反应详情

A solution of 5-amino-2-methoxypyridine (2.48 g, 20.0 mmol) and N-ethyldiisopropylamine (2.84 g, 22.0 mmol) in dichloromethane (20 ml) was cooled in an ice-bath. Benzoyl chloride (3.09 g, 22 mmol) was slowly added by means of a syringe. The cooling bath was removed and stirring was continued at room temperature for 18 hours. Dichloromethane was added and the solution was extracted with water. The organic layer was dried over sodium sulphate, filtered and evaporated in vacuo leaving a dark solid. Crystallisation from ethyl acetate:heptane yielded the title compound (3.44 g, 75% yield).

1. customThe cooling bath was removed
2. additionDichloromethane was added
3. extractionthe solution was extracted with water
4. dry with materialThe organic layer was dried over sodium sulphate
5. filtrationfiltered
6. customevaporated in vacuo
7. customleaving a dark solid
8. customCrystallisation from ethyl acetate